Mechanical alloying of MoSi2 with ternary alloying elements. Part 1: Experimental

Phase evolution during the mechanical alloying of Mo and Si elemental powders with a ternary addition of Al, Mg, Ti or Zr was monitored using X-ray diffraction. Rietveld analysis was used to quantify the phase proportions. When Mo and Si are mechanically alloyed in the absence of a ternary element, the tetragonal C11b polymorph of MoSi2 (t-MoSi2) forms by a self-propagating combustion reaction. With additional milling, the tetragonal phase transforms to the hexagonal C40 structure (h-MoSi2). The mechanical alloying of Al, Mg and Ti additions with Mo and Si tend to promote a more rapid transformation of t-MoSi2 to h-MoSi2. In high concentrations, the addition of these ternary elements inhibits the initial combustion reaction, instead promoting the direct formation of h-MoSi2. The addition of Zr tends to stabilise the tetragonal phase.

Limitations of asymmetric parallel-beam geometry

Bragg diffraction peak profiles and intensities in asymmetric (Omega-2theta) diffraction using a mirror-based parallel-beam geometry were compared with symmetric parallel-beam (theta-2theta) and conventional Bragg - Brentano (theta-2theta) diffraction for a powdered quartz sample and the NIST standard reference material (SRM) 660a (LaB6, lanthanum hexaboride). A comparison of the intensities and line widths (full width at half-maximum, FWHM) of these techniques demonstrated that low incident angles (Omega < 5&DEG;) are preferable for the parallel-beam setup. For higher &UOmega; values, if 2θ < 2Omega, mass absorption reduces the intensities significantly compared with the Bragg - Brentano setup. The diffraction peak shapes for the mirror geometry are more asymmetric and have larger FWHM values than corresponding peaks recorded with a Bragg - Brentano geometry. An asymmetric mirror-based parallel-beam geometry offers some advantages in respect of intensity when compared with symmetric geometries, and hence may be well suited to quantitative studies, such as those involving Rietveld analysis. A trial Rietveld refinement of a 50% quartz - 50% corundum mixture was performed and produced adequate results.